CN103674635A - Dose-based end-pointing for low-kV FIB milling TEM sample preparation - Google Patents

Dose-based end-pointing for low-kV FIB milling TEM sample preparation Download PDF

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CN103674635A
CN103674635A CN201310386836.5A CN201310386836A CN103674635A CN 103674635 A CN103674635 A CN 103674635A CN 201310386836 A CN201310386836 A CN 201310386836A CN 103674635 A CN103674635 A CN 103674635A
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thin layer
ion beam
focused ion
low energy
milling
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CN103674635B (en
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T.G.米勒
J.阿加瓦奇
M.莫里亚蒂
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FEI Co
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    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F1/00Etching metallic material by chemical means
    • C23F1/02Local etching
    • C23F1/04Chemical milling
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/32Polishing; Etching
    • GPHYSICS
    • G03PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03FPHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F1/00Originals for photomechanical production of textured or patterned surfaces, e.g., masks, photo-masks, reticles; Mask blanks or pellicles therefor; Containers specially adapted therefor; Preparation thereof
    • G03F1/68Preparation processes not covered by groups G03F1/20 - G03F1/50
    • G03F1/72Repair or correction of mask defects
    • G03F1/74Repair or correction of mask defects by charged particle beam [CPB], e.g. focused ion beam
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/302Controlling tubes by external information, e.g. programme control
    • H01J37/3023Programme control
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/304Controlling tubes by information coming from the objects or from the beam, e.g. correction signals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/30Electron-beam or ion-beam tubes for localised treatment of objects
    • H01J37/305Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching
    • H01J37/3053Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching
    • H01J37/3056Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating or etching for evaporating or etching for microworking, e.g. etching of gratings, trimming of electrical components
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30Electron or ion beam tubes for processing objects
    • H01J2237/304Controlling tubes
    • H01J2237/30466Detecting endpoint of process
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30Electron or ion beam tubes for processing objects
    • H01J2237/317Processing objects on a microscale
    • H01J2237/3174Etching microareas
    • H01J2237/31745Etching microareas for preparing specimen to be viewed in microscopes or analyzed in microanalysers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/30Electron or ion beam tubes for processing objects
    • H01J2237/317Processing objects on a microscale
    • H01J2237/31749Focused ion beam

Abstract

A method, system, and computer-readable medium for forming transmission electron microscopy sample lamellae using a focused ion beam including directing a high energy focused ion beam toward a bulk volume of material; milling away the unwanted volume of material to produce an unfinished sample lamella with one or more exposed faces having a damage layer; characterizing the removal rate of the focused ion beam; subsequent to characterizing the removal rate, directing a low energy focused ion beam toward the unfinished sample lamella for a predetermined milling time to deliver a specified dose of ions per area from the low energy focused ion beam; and milling the unfinished sample lamella with the low energy focused ion beam to remove at least a portion of the damage layer to produce the finished sample lamella including at least a portion of the feature of interest.

Description

The end points based on dosage for low kV FIB milling in TEM sample preparation is determined
Technical field
The present invention relates to the preparation for the sample of transmission electron microscopy (TEM) or scanning transmission electron microscopy (STEM), and relate to particularly the use of charged particle beam in preparation TEM or STEM sample.
Background technology
Transmission electron microscopy (TEM) makes observation person can form nanoscale to the image of the very small feature of the mark level of dust.TEM also allows the inner structure of analytic sample.In TEM, wide electron beam impacts sample and transmission is passed the electronics process focusing of sample with the image of formation sample.Sample must enough thinly penetrate through sample and on opposition side to allow former intrafascicular electronics to advance.
A microscopy for correlation type, scanning transmission electron microscopy (STEM), has similar requirement and ability.
The thin TEM sample cutting from bulk sample material is called as " thin layer ".Thickness of thin layer is less than 100 nanometers (nm) conventionally, but for some application, thin layer must be significantly thinner.With regard to 30 nm and following sophisticated semiconductor manufacture craft, the thickness of thin layer often need to be less than 20 nm, to avoid overlapping between small-scale structure.The variation in thickness of sample can cause thin layer bending, excessive milling or other significant deficiency.For so thin sample, thin layer preparation is a committed step in tem analysis, and it has determined quality and the analysis to minimum and most critical structure of structural characterization to a great extent.
The various milling machine operations that the art methods of preparing for TEM thin layer utilizes focused ion beam (FIB) system to carry out conventionally.This milling machine operation comprises clean xsect, regular cross-section and the frame milling of placing as follows: the drop point of milling pattern is determined the final position at the edge of thin layer.The degree of accuracy of the drop point of the degree of accuracy of thickness of thin layer and final thin layer center based on these FIB milling machine operations.In automatically working flow process, conventionally about a certain feature or reference point on the top surface of substrate that from it will milling TEM sample, carry out all millings.
Shown in Figure 10 A to Figure 10 I, for example, in transferring U.S. Patent number 20130143412 A1 of assignee of the present invention FEI Co. " for the preparation of the method (Methods for Preparing Thin Samples for TEM Imaging) of the thin sample for TEM imaging ", a kind of art methods of preparing thin TEM sample has been described.In Figure 10 A, described to complete the vertical sample in cross section 1002 after bulk milling.Vertical sample in cross section 1002 is attached in the bulk substrate at side and place, bottom, but for clarity, does not demonstrate bulk substrate around.In Figure 10 B, described excessive milling district 1052, these excessive milling districts have typically shown hanging to a certain degree.Use ion beam 1706 to thin sample in cross section 1002 on the first side 1051A.
In Figure 10 C and Figure 10 D, added material 1056, thereby made to increase the gross thickness in raw sample cross section 1002.Remove alternatively the material 1056 that part is added.It is upper that sufficient deposition materials 1056 has been stayed sample face 1051A, and additional structural integrity is provided during with another sample face of convenient milling 1051B.In Figure 10 E, before final sample face 1051B exposes, additional materials 1056 can deposit on sample 1002.Then, follow-up additional thinning in process, can remove deposition materials 1056.
Then, in Figure 10 F, at the 2nd TEM sample face 1051B(dorsal part of sample 1002) locate to guide FIB 1706 to thin this sample.The the second sample face 1051B exposing, by conventionally also showing hanging to a certain degree, causes excessive milling district 1052.In Figure 10 G and 10H, use suitable method (as chemical vapour deposition) also to make material 1056 deposit on the second sample face 1051B.Then the some or all of deposition materials on removing second by FIB milling.In Figure 10 I, can alternatively all deposition materials 1056 be removed from completed TEM sample 1010.
Known problem about the production of crystalline material (silicon is commercially important example) thin layer is, high-energy focusing ion beam (for example, 30 kiloelectron-volts (keV)) is producing substantial breakable layer in final thin layer.For example by the energetic ion of upsetting the lattice of sample, cause breakable layer.Known solution, for to carry out some final procedure of processings under lower FIB energy, typically is 2 keV to 5 keV, but is conventionally not more than 8 keV.These lower FIB energy procedure of processings are often called as " destroy and remove " step.In some cases, even use lower landing energy (being less than 2 keV).Conventionally, landing energy is lower, and the upset of lattice is less, and result breakable layer thickness is along with landing energy reduces and reduces.
The operation of low landing energy is sometimes also referred to as low kV operation, this be because, if sample under earth potential, landing energy is directly relevant to the high voltage potential on ion gun tip.
To low kV(kilovolt) to destroy the relevant problem of clear program and be, FIB resolution and probe feature are greatly demoted under low kV.Because under low kV, aberration causes probe formation usefulness greatly to be demoted conventionally, so FIB resolution and probe feature are demoted.
This means relate to imaging in steps (as destroyed for placing final low kV the step of removing milling) there is the ability of having demoted.Typically, the thin layer that robotization processing produces, wherein, the drop point of low kV milling has critical impact to final cutting drop point and thickness and precision.Net result is, much better at low kV at the control ratio of the drop point of 30 kV lower limbs, and destroys reset procedure and introduce undesirably a large amount of uncertain to the thickness of final thin layer and position.
Summary of the invention
Exemplary embodiment of the present invention comprises a kind of for using focused ion beam to form the method for transmission electron microscopy sample thin layer.The method comprises: by the guiding of high-energy focusing ion beam, to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount; With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer; To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer; After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And one or more with in the exposure of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
Another exemplary embodiment of the present invention comprises a kind of system that is used to form transmission electron microscopy sample thin layer.This system comprises: focused ion beam post; Example platform; Be placed on example platform or interior sample; Programmable Logic Controller, this controller causes this system automatically to proceed as follows: by the guiding of high-energy focusing ion beam, to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount; With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer; To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer; After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And by one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
Another exemplary embodiment of the present invention comprises a kind of non-transient computer-readable medium by computer program code, this computer program is for automatically forming transmission electron microscopy sample thin layer, this computer program comprises computer instruction, when being carried out by computer processor, these computer instructions cause the computing machine of controlling focused ion beam system to proceed as follows: high-energy focusing ion beam is guided to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount; With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer; To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer; After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And by one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
In order to understand better following detailed description of the present invention, feature of the present invention and technological merit have been summarized quite widely above.Below supplementary features of the present invention and advantage will be described.Those skilled in the art will recognize that disclosed concept and specific embodiment can be easily with the bases that makes improvements or be designed for identical other structures of object of the present invention.Those skilled in the art also will be appreciated that these equivalent constructions do not depart from as the spirit and scope of the present invention as illustrated in the claim of enclosing.
Accompanying drawing explanation
In order to understand more up hill and dale the present invention and advantage of the present invention, now by reference to the accompanying drawings with reference to following explanation, wherein:
Fig. 1 shows the thin layer 104 cutting from sample substrate 102, and this sample substrate is included in thin layer has feature to be analyzed before sample substrate is removed;
Fig. 2 shows the vertical view at thin layer thin layer 104 from sample substrate 102 cuttings before sample substrate is removed;
Fig. 3 shows the vertical view of one end of semi-manufacture thin layer 104, comprises the position of breakable layer 302a and 302b and final thin layer 304;
The drop point that Fig. 4 shows the vertical view of semi-manufacture thin layer 104 and carries out the exemplary DikV milling district 402 of final milling;
Fig. 5 shows the side view of the semi-manufacture thin layer 104 in low kV milling process;
Fig. 6 shows the top-down figure of finished product thin layer 304;
Fig. 7 shows an embodiment who is equipped to the exemplary charged particle beam system 702 of implementing embodiments of the invention;
Fig. 8 shows a process flow diagram, has described a kind of low kV method that end points based on dosage according to one or more embodiment of the present invention determines to form TEM sample thin layer;
Fig. 9 shows a process flow diagram, has described a kind of for one or more embodiment usefulness that improves final milling from the feedback of processing stand according to the present invention; And
Figure 10 A to Figure 10 I has described a kind of art methods for the preparation of thin TEM sample.
Embodiment
Embodiments of the invention are for for utilizing the definite low energy charged particle bundle milling of the end points that has based on dosage to form the method and system of sample thin layer.Some embodiments of the present invention comprise for utilizing the definite low energy charged particle bundle milling of end points having based on dosage to form the full-automatic method and system of sample thin layer.Some embodiments of the present invention comprise the method and system for utilizing robotization step that the operator of instrument carries out and manual step to form sample thin layer.In at least one embodiment, charged particle beam is that focused ion beam and sample thin layer are transmission electron microscopy (TEM) thin layer and/or scanning transmission electron microscopy (STEM) thin layer.With high precision thin layer edge drop point, carry out the high kV(of standard approximately 30 kV) milling.By standard program, place high kV milling, typically utilize the reference point near the substrate surface of features relevant, at least a portion features relevant will be included in finished product sample thin layer.High kV thickness of thin layer and drop point are determined by base point accuracy problem known in the art.
After accurate high kV milling completes, suitably locate thin layer and thin layer is milled into the thickness of accurate control.Yet the thickness of thin layer is less times greater than expection final thickness, to can remove the breakable layer causing due to high kV milling with final milling.In a preferred embodiment, thin layer is than two double-lengths of the length of the penetration depth of the thick about particle beams for high kV milling of desirable thin layer final thickness.In the example of 30 kV gallium ion beam, penetration depth is approximately 30 nm.
Method based on dosage is used for removing breakable layer.With the pattern of placing as follows, carry out final low kV milling: the precision of milling drop point is inessential, only has final dose important.In a preferred embodiment, with the size larger than thin layer area, carry out " frame " milling.In some cases, the sample from larger is extracted to the thin layer of making, as wafer or wafer piece, wherein near the top surface of sample, have structure.In order to minimize the undesirable artefact with milling some type that thoroughly these structures are associated, what make us wishing is to have an obvious angle between incident particle bundle and the ray perpendicular to the top surface of the sample in the plane of lamina plane.Typically, wish that this angle is greater than 30 (30) degree.In one embodiment, with the top surface with respect to sample, be essentially the angle guiding FIB of 45 degree.Other embodiment comprise that FIB is around the additional rotation of the axle vertical with sample surfaces.Another embodiment comprises and relates to ion beam with respect to the substantive position angle of surface normal and the multiple angle of substantial polar angle again.Can realize these angles with various ways, sometimes relate to multiaxis platform, and sometimes relate to one or more removable posts with desirable fixed orientation.
The accurate Characterization of the material clearance rate providing on lamina plane and the low kV milling that the sign based on material clearance rate is carried out time control are provided the additional aspect of embodiments of the invention.In certain embodiments, the material clearance rate on lamina plane is characterised in that accurate calibration based on beam current determines the exact dose of the charged particle that the low kV particle beams sends.The accurate calibration of beam current is made explanations to the variation of the beam current occurring in a period of time.The function of the beam current when dosage of the charged particle sending is scan area, scanning consuming time and scanning.Typically, maximum uncertainty is associated with ion beam current.For the good control of dosage is provided, with the regular time interval or within the schedule time that approaches the milling based on dosage measure beam current.Can any stipulated time before thin layer preparation carry out this measurement.Several, the milling that can be for example, some minutes of starting last second of milling for the stipulated time of measuring start last minute some minutes several, once a day, once in a week, each wafer one is inferior.The method of calibration FIB electric current, conventionally by ion beam is guided in current collector, by this current collector, is carried out accurate current measurement by accurate current measurement electronic equipment.Can in ion column or on the position beyond ion column, complete this measurement.
Low kV imaging or pattern identification are not depended in the control of removing material, and only depend on the accurate control of final dose.Directly the careful measurement (for example, beam current error is no more than 1%) of the FIB beam current before milling and milling careful control (for example, being no more than 1% timing error) regularly causes the quantity of material error of removing from semi-manufacture thin layer to be no more than 2%.From every side of semi-manufacture thin layer, removing the exemplary cases of 30 nm materials, milling error controls to and is no more than 2% error limitation that low kV milling is caused to being less than a nanometer.The numeral of using in this paragraph is only for illustration purpose.
Calibration beam current is not the sole mode of exosyndrome material clearance rate.In some embodiments of the invention, the sign that material clearance rate under the particle beams condition of used low kV carries out clearance rate is measured on property ground by experiment.For example, can experimentally carry out low kV milling and from lamina plane, remove 1 nm material to determine (for one group of given particle beams condition) per minute.The sign that can any stipulated time before thin layer preparation carry out the experimental measurement of material clearance rate.Several, the milling that can be for example, some minutes of starting last second of milling for the stipulated time of measuring start last minute some minutes several, once a day, once in a week, each wafer one is inferior.
In another preferred embodiment of the present invention, from the feedback of processing stand can with regularly and dosage control combine and maybe can be used to timing and the suitable value of dose determination.For example, according to embodiments of the invention, producing in the process of one or more thin layers, based in thin layer production run, careful control regularly of milling and the amount that the monitoring of actual beam current is sent to the dosage of each thin layer in to thin layer production run being carried out to accurate record.Observe subsequently thin layer and realize its target object degree to determine processing, and this information is fed back in system to regulate the target dose for the production of additional thin layer.Can be undertaken this by any practical approach and check, comprise system SEM image in the instrument thinning for low kV or the information of collecting from produce the TEM of the final image of thin layer or STEM system.Machine vision algorithm can, for measuring the feature of thin layer, be ready to use in to calculate the pondage factor of determining subsequent dose.
In another example, run through the whole process that completes of high kV operation, system is processed a plurality of samples.Then, this system thins operational applications on a subset sample and collect and the information of the same number of above-mentioned example by low kV.This instrument is collected SEM image and the personnel inspection quality results of finished product thin layer.Which type of conversion factor personnel can indicate to be sent on left point.Alternately, machine vision algorithm can, for measuring the feature of thin layer, be ready to use in to calculate the pondage factor of determining subsequent dose.When producing follow-up thin layer, the information based on SEM image check combines to reduce with the beam current of preparing the new actual measurement on instrument the actual dose sending to unit area, so that realize target thickness of sample more accurately.
Embodiments of the invention are particularly useful to form TEM sample thin layer with monocrystal material (as silicon).Monocrystal substrate is subject to the larger destruction of substrate being formed by monocrystal than not being, those as used in data-storage applications in high kV milling process.
Fig. 1 shows at thin layer semi-manufacture thin layer 104 from sample substrate 102 cuttings before sample substrate is removed.By milling away material from sample substrate 102 on the surrounding position at thin layer, form semi-manufacture thin layer 104.Use charged particle beam milling of materials, as ion beam, electron beam or laser beam.In a preferred embodiment, charged particle beam is focused ion beam.One or more reference point (not shown) in sample substrate 102 can be for locating desirable coating position.First with high precision thin layer edge drop point, carry out the high kV milling of standard.High kV milling use have be greater than 8 keV preferably the charged particle beam of approximately 30 keV from sample substrate, remove material.
Fig. 2 shows the vertical view that carries out the semi-manufacture thin layer 104 after initial high kV milling.Charged particle beam is removed base material from GaokV milling district 202a and 202b, to expose vertical thin aspect 204a and 204b. GaokV milling district 202a and 202b are positioned at the both sides of thin layer 104.One or more reference point (not shown) can be for the GaokV milling district 202a in definite sample substrate and the position of 202b.Because high kV milling is for from GaokV milling district 202a and 202b removing material, so being included in thin layer, semi-manufacture thin layer 104 can before tem analysis for example, be needed the breakable layer that is corrected or removes.
Fig. 3 shows the vertical view of one end of semi-manufacture thin layer 104, comprises the position of breakable layer 302a and 302b and final thin layer 304. Breakable layer 302a and 302b extend to a certain degree of depth in semi-manufacture thin layer 104 from lamina plane 204a and 204b.In order to allow to remove breakable layer in follow-up low kV milling step, carry out high kV milling step, make semi-manufacture thin layer 104 there is the thickness larger than the expection thickness of final thin layer 304.In one or more embodiments, carry out high kV milling, thereby make each limit of thin layer 104 substantially than thick 30 nanometers of the expection thickness on the limit of finished product thin layer 304 (nm).
Breakable layer 302a and 302b are caused by the initial high kV milling of semi-manufacture thin layer 104.With beam of high energy charged particles milling, there is the higher and more accurate benefit of particle beams drop point of milling rate, because reduced aberration.But high energy particle also damages sample substrate, produce breakable layer 302a and 302b.For example, by focused ion beam, silicon crystal substrate is carried out to high kV milling meeting lattice is caused to undesired destruction.Therefore, embodiments of the invention comprise and carry out final milling to remove breakable layer 302a and 302b.The low kV milling that final milling step is determined for the end points utilizing based on dosage.
The drop point that Fig. 4 shows the vertical view of semi-manufacture thin layer 104 and carries out the exemplary DikV milling district 402 of final milling.Place as follows in DikV milling district 402: the precision of drop point is inessential, and the final dose that only has particle is important.Preferably, with the larger size of the expection final thickness than finished product thin layer 304, in the surrounding of semi-manufacture thin layer 104, carry out frame milling.The frame milling of simple types is for wherein describing snakelike or comb mesh pattern and repeatedly replotting goes out this pattern within the milling duration milling across the geometric configuration (typically being rectangle) of definition.For purposes of the present invention, key is that the difference of frame milling and clean xsect milling is that clean cross section type milling has slowly progressive milling position.For purposes of the present invention, the exact details of frame milling pattern is inessential, for example, can depict pattern across being essentially circular definition.DikV milling district 402 consists essentially of all breakable layer 302a and 302b, thereby once make to complete low kV milling machine operation just substantially from finished product thin layer 304 supernatants except all breakable layer 302a and 302b.Because used low kV milling rather than high kV milling, so compare with the destruction of semi-manufacture thin layer 304 being caused due to high kV milling, eliminated or significantly reduced the destruction to finished product thin layer 304.
Fig. 5 shows the side view of the semi-manufacture thin layer 104 in low kV milling process.Can be by not being that the mode of " top-down " operates charged particle beam and improves usefulness substantially.In some cases, the sample from larger is extracted to thin layer 104, as wafer or wafer piece, wherein near the top surface of sample 102, have structure.In order to minimize the undesirable artefact with milling some type that thoroughly these structures are associated, what make us wishing is to have an obvious angle (θ) between incident particle bundle and the ray 504 perpendicular to the top surface of the sample in the plane of thin layer 104.Typically wish that this angle θ is greater than 30 (30) degree.In one embodiment, with the top surface with respect to sample, be essentially the angle θ guiding FIB of 45 degree.
Fig. 6 shows the top-down figure of finished product thin layer 304.By carry out low kV milling substantially from finished product thin layer 304 supernatants except all breakable layer 302a and 302b.In the bottom of finished product thin layer, finished product thin layer 304 may still be attached in sample substrate 102.Can (as undercut) for further processing, to thin layer 304 and sample substrate are separated, at another instrument inner analysis.
Fig. 8 shows a process flow diagram, has described a kind of low kV method that end points based on dosage according to one or more embodiment of the present invention determines to form TEM sample thin layer.The method starts at 802 places and proceeds to step 804, in step 804, at sample substrate 102 places, guides beams of high energy charged particles.Beam of high energy charged particles is guided to sample substrate 102 to be sentenced and carries out high kV milling machine operation.High kV milling machine operation is used energetic particle beam that the bulk substrate material of unnecessary amount is removed from GaokV milling district 202a-202b, to expose semi-manufacture thin layer 104(step 806) vertical thin aspect 204a and 204b.Beam of high energy charged particles has the landing energy that is greater than 8 keV, and is preferably about 30 keV.
Destroying before removing with low energy particle Shu Jinhang, the material clearance rate of low energy charged particle bundle is characterized to (step 808).Can be by accurate measure beam current determining beam current after calibration, measure to property by experiment the material clearance rate of low energy particle bundle or by any other suitable sign of clearance rate that completes for characterizing the method for the clearance rate of low energy particle bundle.If clearance rate is characterized by measure beam current, by explaining that the accurate calibration of the beam current that change the every day (or even more continually) of beam current controls the dosage of charged particle.In one embodiment of the invention, the beam current directly carry out step 808 before carrying out low kV milling step in is measured.Alternately, the beam current in can carry out step 808 under the time interval separating is regularly measured.The method of calibration beam current includes but not limited to measure the blanking particle beams and use desk-top Faraday cup measure beam current with calibrated micromicroammeter.
With after beam of high energy charged particles milling semi-manufacture thin layer 104 and after material clearance rate is characterized, low energy charged particle bundle is guided to semi-manufacture thin layer 104(step 810).This low energy charged particle bundle has the landing energy that is less than 8 keV, and preferably between 2 keV and 5 keV.Low energy charged particle bundle is guided to semi-manufacture thin layer 104 to be sentenced and carries out low kV milling machine operation.Low kV milling machine operation is used low energy particle bundle to remove breakable layer 302a and 302b(step 812).This low-kV milling step is by accurate timing, thereby makes to send based on milling time and materials clearance rate the charged particle (step 814) that pre-determines dosage.When sending the charged particle that pre-determines dosage, the method stops at terminating symbol 816 places.Finished product thin layer comprises at least a portion features relevant.
Low-kV imaging or pattern identification do not depended in the control of removing material, and only depends on the accurate control of final dose.Final dose is controlled in material clearance rate during stipulated time by accurate Characterization before milling and the timing of carefully controlling milling.In a preferred embodiment, timing error is controlled to and be less than one of percentage (1%) and the error of beam current is controlled to and is less than one of percentage (1%).This causes the error of the material that is eliminated to be less than (2%) 2 percent.For example, if remove the material of 30 nanometers (30 nm) in each side of semi-manufacture thin layer 104, the control of material being eliminated is caused to Ya Na meter error to being less than the low kV milling machine operation of 2% permission.
The present invention has been described about forming the embodiment of TEM thin layer herein.Those skilled in the art will recognize that, embodiments of the invention are not only confined to form TEM thin layer, but also are applicable to the thin layer of other types, as STEM thin layer.
In a preferred embodiment, the method in Fig. 8 is full-automatic, and the final end points of finished product thin layer 304 is determined mutual without any need for people, particularly anyone visual interactive.Direct measure beam current before low-kV milling step, and the beam current calibration adjustments based on up-to-date low-the kV milling time, to provide split-hair dosage, control.Place as follows milling pattern: " over-exposure goes out " domain of dependence region around, thus make the position of drop point there is slight influence or not impact to the material of removing from domain of dependence.
Fig. 9 shows a process flow diagram, has described a kind of use and from the feedback of processing stand, has improved the method for the usefulness of final milling.In this embodiment of the present invention, from the feedback of processing stand can with regularly and dosage control combine and maybe can be used to timing and the suitable value of dose determination.The step 904 that the method starts and carries out at frame 902 places.According to the method in Fig. 8, produce first group of one or more thin layer.Based in thin layer production run to careful control regularly of milling with the monitoring of actual beam current is carried out to accurate record to being sent to the amount of the dosage of each thin layer in step 904 process.Observe subsequently thin layer and realize its target object degree to determine processing.Or one or more features (step 906) of the point in time measurement thin layer when milling thin layer or after complete lamellar milling just.Record one or more features (step 908) of thin layer, if thickness of thin layer, the residue size of breakable layer are, the error deviation of milling drop point etc.The second prescribed dose (step 910) of the ion of the difference calculating low energy focused ion beam unit area between the one or more features based on expection thin layer feature and measured this first group of thin layer.This information is fed back in system to regulate the target dose for the production of additional thin layer.Can be undertaken this by any practical approach and check, comprise system SEM image in the instrument thinning for low kV or the information of collecting from produce the TEM of the final image of thin layer or STEM system.The second pattern milling time of the second prescribed dose of applying unit area transmission low energy focused ion beam is produced second group of one or more sample thin layer (step 912).This process finishes at terminating symbol 914 places.Can repeatedly apply this feedback procedure to improve the precision of finished product sample thin layer milling.
For example, use the embodiment of the method for Fig. 8 and Fig. 9, produce following many information of systematic collection of thin layer: (1) is before starting low kV milling, thickness of sample is 95.0 nm, (2) under the accelerating potential of 2 kV, carry out low kV milling, (3) are sent to 9.00 μ m by the low kV milling of applying in every side 2the target area duration of 35.7 seconds that area is large, and (4) are 85.4 pA at measured beam current of the time of low kV milling.Make the TEM system of thin layer imaging determine that thickness of sample is less by 4% than optimum thickness.When producing follow-up thin layer, from the information of TEM system, combine to reduce the actual dose of unit area transmission with the beam current of preparing the new actual measurement on instrument, so that realize target thickness of sample more accurately.
In another example, run through the whole process that completes of high kV operation, system is processed a plurality of samples.Then, this system thins operational applications on a subset sample and collect and the information of the same number of above-mentioned sample by low kV.This instrument is collected SEM image and the personnel inspection quality results of finished product thin layer.Which type of conversion factor personnel can indicate to be sent on left point.When producing follow-up thin layer, the information based on SEM image check combines to reduce the actual dose of unit area transmission with the beam current of preparing the new actual measurement on instrument, so that realize target thickness of sample more accurately.
Fig. 7 has described to be equipped to an embodiment of the exemplary two-beam SEM/FIB system 702 of implementing embodiments of the invention.The present invention does not need double-beam system, but can easily use together with any charged particle beam system, comprises single FIB system.Double-beam system described herein is only for exemplary purpose.Can in two-beam electron beam/focused ion beam system (as the system as described in now), carry out preparation and the analysis of this TEM sample.For example can be purchased suitable charged particle beam system from Ore. Hillsborough FEI Co. of assignee of the present invention.Although the example of suitable hardware is below provided, has the invention is not restricted to be implemented with the hardware of any particular type.
Double-beam system 702 has vertically arranged electron beam column 704 and becomes focused ion beam (FIB) post 706 of about 52 degree angles installations with the vertical line with finding time on sample chamber 708.Can be by pumping system 709 sample chamber of finding time, this pumping system generally includes one or more in turbomolecular pump, ODP, ion getter pump, vortex pump or their combination, or other known pumping installations.
Electron beam column 704 comprises for generation of the electron source 710(Schottky emitter of electronics or awkward silence at a meeting transmitter) and the electro- optical lens 712 and 714 that forms electronic features focused beam acts 716.Electron source 710 remains on above 500 V of current potential of workpiece 718 and the current potential between 30 kV conventionally, and this workpiece remains on earth potential conventionally.
Therefore, electronics impacts workpiece 718 with about 500 eV to the landing energy of 30 keV.Can on this workpiece, apply negative potential, to reduce the landing energy of electronics, this has reduced the total electron amount mutual with this workpiece, thereby has reduced the size in nucleation site.Workpiece 718 for example can comprise semiconductor device, MEMS (micro electro mechanical system) (MEMS), data storage device or for analyzing the sample of the material of its material characteristics or composition.Can the shock point of electron beam 716 be positioned at by deflection coil 720 on the surface of workpiece 718 or the shock point of scanning beam 716 thereon.By scanning electron microscope power supply and control module 722, control lens 712 and 714 and the operation of deflection coil 720.Lens and deflection unit can be used electric field, magnetic field or its combination.
On the moveable platform 724 of workpiece 718 in sample chamber 708.Platform 724 can be preferably (Z axis) mobile and about 60 (60) degree and rotating around Z axis of can tilting in horizontal plane (X-axis and Y-axis) and vertically.Can open door 727 to workpiece 718 is inserted on X-Y-Z platform 724 and is convenient to keep in repair inner air feed tank (if use air feed tank) (not shown).This quilt is interlocked, thereby if sample chamber 708 is evacuated, door can not be opened.
One or more gas ejecting systems (GIS) 730 are arranged on vacuum chamber.Each GIS can comprise for being installed in the storage tank (not shown) of precursor or activated material and for gas being guided to the lip-deep pin 732 of workpiece.Each GIS further comprises for regulating to the device 734 of workpiece supply precursor material.In this example, depict this regulating device as adjustable valve, but this regulating device can also comprise for example for precursor material being heated to control the adjusting well heater of its vapor pressure.
When the electron bombardment workpiece 718 of electron beam 716, transmitting also can detect electronic secondary, backscattering electronics and Auger (Auger) electronics, to form image or to determine the information about this workpiece.For example electronic secondary by secondary electron detector 736(as Everhart-Thornley detecting device) or the semiconductor detector device that can be detected low-energy electron detect.The STEM detecting device 762 that is positioned at TEM sample holder 761 and platform 724 belows can be collected transmission by being arranged on the electronics of the sample on this TEM sample holder.Come the signal of self-detector 736,762 to be provided to programmable system controller 738.Described controller 738 is also being controlled other objects of deflector signal, lens, electron source, GIS, platform and pump and instrument.Watch-dog 740 is for using signal to show that user controls and the image of workpiece.Described controller 738 can comprise general programmable computing machine, this computing machine comprises tangible non-transient computer-readable medium, with computer instruction, this storer is encoded, when being carried out by the processor of computing machine, these instructions cause this computer automatic execution embodiments of the invention, as the method for describing in Fig. 8.
Under the control of vacuum controller 741, by pumping system 709 evacuated chambers 708.This vacuum system provides about 7 * 10 in chamber 708 -6the vacuum of mbar.When suitable precursor or activator gas are introduced on sample surfaces, chamber background pressure can rise, and conventionally rises to approximately 5 * 10 -5mbar.
Focused ion beam post 706 comprises that neck 744(ion gun 746 is positioned at wherein) and focus on post 748, this focusing post comprises extraction electrode 750 and electrostatic optics system, this electrostatic optics system comprises object lens 751.Ion gun 746 can comprise the ion gun of liquid metal gallium ion source, plasma ion source, liquid metal alloy source or any other type.The axle that focuses on post 748 can be with becoming non-zero angle to be directed with the axle of electron beam.Ion beam 752 leads to workpiece 718 between ion gun 746 line focus posts 748 and static deflecter 754.
FIB power supply and control module 756 provide current potential at ion gun 746 places.Ion gun 746 remains on above 1 kV of current potential of workpiece and the current potential between 60 kV conventionally, and this workpiece remains on earth potential conventionally.Therefore, ion lands energy impact workpiece with about 1 kV to 60 kV.FIB power supply and control module 756 are coupled on deflecting plate 754, and these deflecting plate can cause ion beam on the upper surface of workpiece 718, to depict corresponding pattern.In some systems, as known in the art, deflecting plate is placed on before last lens.When FIB power supply and control module 756 are when applying blanking voltage on blanking electrode, the beam blanking electrode (not shown) in ion beam focusing post 748 causes ion beam 752 to impact on blanking aperture (not shown) rather than workpiece 718.
Ion gun 746 provides a branch of conventionally can be focused at workpiece 718 places the gallium particle of the only positively charged of 1/10th sub-micron wide beams, to workpiece 718 is modified, or to made workpiece 718 imagings by ion milling, enhancing etching, deposition of material.
Micro-manipulator 757(is as the MM3A model of the automatic prober 200 of Texas, USA Dallas Omniprobe company or Germany Reutlingen Kleindiek Nanotechnik) can be in vacuum chamber mobile object accurately.Micro-manipulator 757 can comprise the precision motor 758 being positioned at outside vacuum chamber, to provide X, Y, Z and the Sai Ta of the part 759 that is positioned at vacuum chamber to control.Micro-manipulator 757 can be equipped with the different end effectors for manipulation of small objects.In described embodiment, end effector is a mandrin 760 herein.As known in this area, micro-manipulator (or microprobe) can be for being transferred to TEM sample (it separates with substrate by ion beam conventionally) on TEM sample holder 761, for analysis.
System controller 738 is controlled the operation of the various parts of double-beam system 702.By system controller 738, user can cause ion beam 752 or electron beam 716 to scan in desirable mode via the instruction inputing in conventional user interface (not shown).Alternately, system controller 738 can be controlled double-beam system 702 according to programming instruction.Fig. 7 is indicative icon, and it does not comprise all elements and its actual look that does not reflect all elements and size and the relation between them of typical double-beam system.
Although above explanation of the present invention mainly for the method for the ultra-thin TEM sample of preparation, will be appreciated that the operation of this method of execution will be further within the scope of the invention.Further, will be appreciated that embodiments of the invention can be realized, or be realized by the computer instruction being stored in non-transient computer-readable memory by computer hardware, both combinations of hardware and software.Can in the computer program that uses standard program technology, carry out these methods according to the method described in this instructions and accompanying drawing, comprise the non-transient computer-readable recording medium that disposes computer program, wherein so the storage medium of configuration causes computing machine to operate in specific and predefined mode.Can carry out each program with advanced procedures programming language or Object-Oriented Programming Language.Yet, if wished, can carry out these programs by assembly language or machine language.Under any circumstance, language can be compiling type language or interpreted languages.In addition, program can be moved on this object special IC being programmed for.
Further, can be in the computing platform of any type manner of execution opinion, the computer platform that include but not limited to personal computer, microcomputer, main frame, workstation, networking or distributed computing environment, separates, integrates or communicate by letter with charged particle instrument or other imaging devices etc.Can carry out various aspects of the present invention by the machine readable code being stored on storage medium or device (be no matter dismountable or integrate with computing platform), as hard disk, optically read and/or write storage medium, RAM, ROM etc., thereby make to be read by programmable calculator, while reading this storage medium or device with convenient computing machine, this computing machine is configured and is operated, to carry out program described herein.In addition, can be by the each several part of wired or wireless Internet Transmission machine readable code or machine readable code.Invention described herein comprises these types and other various types of computer-readable recording mediums, and this type of medium comprises for instruction and program in conjunction with microprocessor or other data processors execution above-mentioned steps simultaneously.The present invention also comprises the computing machine itself while being programmed according to method described herein and technology.
Computer program can be applied in input data, to carry out function described herein, thereby and conversion input data turn to generate output data.Output information is applied on one or more output units, as display monitor.In a preferred embodiment of the invention, data representation physics and the visible object changed, be included in the concrete visual depiction that produces physics and visible object on display.
In order to use the particle beams to make sample imaging, the preferred embodiments of the present invention have also been utilized particle beam apparatus, as FIB or SEM.This for making particle and the sample of sample imaging carry out inherence interaction, cause physical deformation in a way.Further, run through this instructions, the discussion of the terms such as use as " calculating ", " determining ", " measurement ", " generation ", " detection ", " formation " is also applicable to handle and the data-switching that is expressed as physical quantity in computing machine become to the computer system of other data that are expressed as similarly physical quantity in computer system or action and the process of like or other information storages, transmission or display device.
The present invention there is broad applicability and can provide as in the example above described and shown in many benefits.According to application-specific, embodiment can alter a great deal, but be not each embodiment can provide be beneficial to and meet all targets that can realize in the present invention.Being applicable to implement particle beam system of the present invention for example can be purchased from assignee FEI formula of the present invention.
Although most of description is for semiconductor wafer before, the present invention can be applied to any suitable substrate or surface.Further, the present invention can be applied to except the sample thinning in vacuum chamber (style product outside the venue) beyond substrate is eliminated vacuum chamber or the sample (on-the-spot style product) being thinned after being applied on substrate extraction the TEM grid in being arranged on vacuum chamber.No matter when use term " automatically ", " robotization " or similar terms herein, those terms will be understood as that and comprise and manually booting automatically or automation process or step.In the following discussion and in claims, in open mode, use term " to comprise " and " comprising ", and therefore should be interpreted as representing " including but not limited to ... ".Term " integrated circuit " refer to one group of electronic unit and they on the surface of microchip, be patterned interconnect (general designation internal circuit element).Term " semiconductor device " typically refers to integrated circuit (IC), this integrated circuit can be incorporated on semiconductor wafer, with wafer-separate or packed being used on circuit board.Term as used herein " FIB " or " focused ion beam " refer to the ion beam of any collimation, comprise the bundle and the shaping ion beam that by ion optics, focus on.
Just in this instructions, do not define specially any term, object is to provide the simple and common meaning of term.Accompanying drawing is intended to help to understand the present invention, and except as otherwise noted, otherwise not to scale (NTS) is drawn.
According to some embodiments of the present invention, a kind of for form the method for transmission electron microscopy sample thin layer by focused ion beam, the method comprises: high-energy focusing ion beam is guided to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount; With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more faces of this semi-manufacture sample thin layer comprise breakable layer; To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer; After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And by one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
In certain embodiments, the material clearance rate that characterizes this low energy focused ion beam further comprises to be measured the beam current of this low energy focused ion beam and determines the beam current after calibration.In certain embodiments, the dosage of unit area ion depends on the area in region at beam current after calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
In certain embodiments, the material clearance rate that characterizes this low energy focused ion beam further comprises that experimentally measures the material clearance rate of this low energy focused ion beam.
In certain embodiments, from same focused ion beam post, launch this high-energy focusing ion beam and this low energy focused ion beam.
In certain embodiments, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV) or is more than or equal to 30 kiloelectron-volts (30 keV).
In certain embodiments, this low energy focused ion beam has and is less than eight kiloelectron-volts (8 keV) or the landing energy between 2 kiloelectron-volts and 5 kiloelectron-volts (2 keV to 5 keV).
In certain embodiments, in the situation that there is no manual intervention, use this low energy focused ion beam milling semi-manufacture sample thin layer.
In certain embodiments, not guide this focused ion beam with the parallel plane angle of thin layer, or with the incident angle of non-zero degree, guide this focused ion beam with respect to the plane of thin layer, or with the angles of 45 (45) degree substantially, guide this focused ion beam with respect to the plane of thin layer, or before milling semi-manufacture sample thin layer, make this focused ion beam or make this sample or make the two around the axle rotation vertical with sample surfaces.
In certain embodiments, this substrate comprises monocrystal material, as silicon.
According to some embodiments of the present invention, the method further comprises: produce first group of one or more thin layer, each thin layer in this group receives the first prescribed dose ion that low energy focused ion beam unit area sends, time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards, record one or more features of this measured first group of thin layer, difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area, the second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
In certain embodiments, personnel manually observe one or more features of this first group of thin layer, and these personnel provide the pondage factor using calculating the second prescribed dose.
In certain embodiments, one or more features of this first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating at the pondage factor of determining that the second prescribed dose is used.
According to some embodiments of the present invention, a kind of system that is used to form transmission electron microscopy sample thin layer, this system comprises: focused ion beam post, example platform, be placed on example platform or interior sample, Programmable Logic Controller, this controller causes this system automatically to proceed as follows: high-energy focusing ion beam is guided to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount, with this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more faces of this semi-manufacture sample thin layer comprise breakable layer, to low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer, after the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam, and by one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
In certain embodiments, this system characterizes the material clearance rate of this low energy focused ion beam by the material clearance rate of measuring the beam current of this low energy focused ion beam and determine the beam current after calibration or measure to property by experiment this low energy focused ion beam.
In certain embodiments, the dosage of unit area ion depends on the area in region at beam current after calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
In certain embodiments, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV).
In certain embodiments, this low energy focused ion beam has and is less than eight kiloelectron-volts (8 keV) or the landing energy between 2 kiloelectron-volts and 5 kiloelectron-volts (2 keV to 5 keV).
In certain embodiments, Programmable Logic Controller further causes this system automatically to produce first group of one or more thin layer, each thin layer in this group receives the first prescribed dose ion that low energy focused ion beam unit area sends, time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards, record one or more features of this measured first group of thin layer, difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area, the second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
In certain embodiments, personnel manually observe one or more features of first group of thin layer, and these personnel provide the pondage factor using calculating the second prescribed dose.
In certain embodiments, one or more features of first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating at the pondage factor of determining that the second prescribed dose is used.
Another exemplary embodiment of the present invention comprises a kind of non-transient computer-readable medium by computer program code, this computer program is for automatically forming transmission electron microscopy sample thin layer, this computer program comprises computer instruction, when being carried out by computer processor, these computer instructions cause the computing machine of controlling focused ion beam system to proceed as follows: high-energy focusing ion beam is guided to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount; With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer; To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer; After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam, and by one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove at least a portion breakable layer, produce thus the finished product sample thin layer that comprises at least a portion features relevant.
In certain embodiments, computer instruction causes the computing machine of controlling focused ion beam system by the material clearance rate of measuring the beam current of this low energy focused ion beam and determine the beam current after calibration or measure to property by experiment this low energy focused ion beam, the material clearance rate of this low energy focused ion beam to be characterized.
In certain embodiments, the dosage of unit area ion depends on the area in region at beam current after calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
In certain embodiments, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV).
In certain embodiments, this low energy focused ion beam has the landing energy that is less than eight kiloelectron-volts (8 keV).
In certain embodiments, computer-readable medium further comprises computer instruction, these computer instructions cause the computing machine of controlling focused ion beam system to proceed as follows: produce first group of one or more thin layer, each thin layer in this group receives the first prescribed dose ion that low energy focused ion beam unit area sends, time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards, record one or more features of this measured first group of thin layer, difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area, the second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
In certain embodiments, personnel manually observe one or more features of first group of thin layer, and these personnel provide the pondage factor using calculating the second prescribed dose.
In certain embodiments, one or more features of first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating at the pondage factor of determining that the second prescribed dose is used.
Although described the present invention and its advantage in detail, it should be understood that and can produce various variations, replacement and change and not deviate from the spirit and scope of the present invention as defined in the claim of enclosing at this.And scope of the present invention is not intended to be limited to the specific embodiment of described in this manual technique, machine, manufacture thing, composition of matter, means, method and step.As those skilled in the art will recognize easily from disclosure of the present invention, can utilize according to the present invention existing or to develop backward, carry out identical function or realize substantially and technique, machine, manufacture thing, composition of matter, means, method or the step of corresponding embodiment identical result described herein substantially.Correspondingly, appended claims is intended in composition, means, method or the step of this type of technique, machine, manufacture thing, material are included in their scope.

Claims (38)

1. for using focused ion beam to form a method for transmission electron microscopy sample thin layer, the method comprises:
By the guiding of high-energy focusing ion beam, to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount;
With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer;
To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before the exposure of this semi-manufacture sample thin layer one or more;
After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And
By one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove this breakable layer of at least a portion, produce thus the finished product sample thin layer that comprises this features relevant of at least a portion.
2. the material clearance rate that the method for claim 1, wherein characterizes this low energy focused ion beam further comprises to be measured the beam current of this low energy focused ion beam and determines the beam current after calibration.
3. method as claimed in claim 2, wherein, the dosage of unit area ion depends on the area in region at beam current after this calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
4. the material clearance rate that the method for claim 1, wherein characterizes this low energy focused ion beam further comprises that experimentally measures the material clearance rate of this low energy focused ion beam.
5. the method as described in claim 1 to 4 any one, wherein, launches this high-energy focusing ion beam and this low energy focused ion beam from same focused ion beam post.
6. the method as described in claim 1 to 4 any one, wherein, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV).
7. the method as described in claim 1 to 4 any one, wherein, this low energy focused ion beam has the landing energy that is less than eight kiloelectron-volts (8 keV).
8. the method as described in claim 1 to 4 any one, wherein, this high-energy focusing ion beam has the landing energy that is more than or equal to 30 kiloelectron-volts (30 keV).
9. the method as described in claim 1 to 4 any one, wherein, this low energy focused ion beam has the landing energy of between two kiloelectron-volts and five kiloelectron-volts (2 keV to 5 keV).
10. the method as described in claim 1 to 4 any one wherein, is used this semi-manufacture sample thin layer of this low energy focused ion beam milling in the situation that there is no manual intervention.
11. methods as described in claim 1 to 4 any one, wherein, not guide this focused ion beam with the parallel plane angle of this thin layer.
12. methods as described in claim 1 to 4 any one, wherein, substrate comprises monocrystal material.
13. methods as claimed in claim 12, wherein, this monocrystal material comprises silicon.
14. methods as described in claim 1 to 4 any one, wherein, guide this focused ion beam with respect to the plane of this thin layer with the incident angle of non-zero degree.
15. methods as claimed in claim 14, wherein, guide this focused ion beam with respect to the plane of this thin layer with the angles of 45 (45) degree substantially.
16. methods as claimed in claim 14, wherein, before this semi-manufacture sample thin layer of milling, make this focused ion beam or make this sample or make the two around the axle rotation vertical with this sample surfaces.
17. methods as described in claim 1 to 4 any one, further comprise:
Produce first group of one or more thin layer, each thin layer in this group receives the ion of the first prescribed dose of this low energy focused ion beam unit area transmission;
Time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards;
Record one or more features of this measured first group of thin layer;
Difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area;
The second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
18. methods as claimed in claim 17, wherein, personnel manually observe one or more features of this first group of thin layer, and these personnel provide the pondage factor using when calculating this second prescribed dose.
19. methods as claimed in claim 17, wherein, one or more features of this first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating the pondage factor using when determining this second prescribed dose.
20. 1 kinds of systems that are used to form transmission electron microscopy sample thin layer, this system comprises:
Focused ion beam post;
Example platform;
Be placed on this example platform or interior sample;
Programmable Logic Controller, this controller causes this system automatically to proceed as follows:
By the guiding of high-energy focusing ion beam, to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount;
With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer;
To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated times before one or more in the exposure of this semi-manufacture sample thin layer;
After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And
By one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove this breakable layer of at least a portion, produce thus the finished product sample thin layer that comprises this features relevant of at least a portion.
21. systems as claimed in claim 20, wherein, this system is by measuring the beam current of this low energy focused ion beam and determining that the beam current after calibration characterizes the material clearance rate of this low energy focused ion beam.
22. systems as claimed in claim 21, wherein, the dosage of unit area ion depends on the area in region at beam current after this calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
23. systems as claimed in claim 20, wherein, this system by experiment material clearance rate of this low energy focused ion beam of property ground measurement characterizes the material clearance rate of this low energy focused ion beam.
24. systems as described in claim 20 to 23 any one, wherein, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV).
25. methods as described in claim 20 to 23 any one, wherein, this low energy focused ion beam has the landing energy that is less than eight kiloelectron-volts (8 keV).
26. methods as described in claim 20 to 23 any one, wherein, this low energy focused ion beam has the landing energy of between two kiloelectron-volts and five kiloelectron-volts (2 keV to 5 keV).
27. methods as described in claim 20 to 23 any one, wherein, this Programmable Logic Controller further causes this system automatically to proceed as follows:
Produce first group of one or more thin layer, each thin layer in this group receives the ion of the first prescribed dose of this low energy focused ion beam unit area transmission;
Time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards;
Record one or more features of this measured first group of thin layer;
Difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area;
The second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
28. systems as claimed in claim 26, wherein, personnel manually observe one or more features of this first group of thin layer, and these personnel provide the pondage factor using calculating this second prescribed dose.
29. systems as claimed in claim 26, wherein, one or more features of this first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating the pondage factor using when determining this second prescribed dose.
30. 1 kinds of non-transient computer-readable mediums by computer program code, this computer program is for automatically forming transmission electron microscopy sample thin layer, this computer program comprises computer instruction, when being carried out by computer processor, these computer instructions cause the computing machine of controlling focused ion beam system to proceed as follows:
By the guiding of high-energy focusing ion beam, to bulk amount material, this bulk amount material comprises the material of features relevant and unnecessary amount, to mill away the material of this unnecessary amount;
With this high-energy focusing ion beam milling, fall the material of this unnecessary amount, to produce the semi-manufacture sample thin layer with the thickness that is greater than desirable finished product sample thickness of thin layer, one or more exposures of this semi-manufacture sample thin layer comprise breakable layer;
To low energy focused ion beam guiding was characterized the material clearance rate of this low energy focused ion beam to the stipulated time before this semi-manufacture sample thin layer;
After the material clearance rate of this low energy focused ion beam is characterized, by the guiding of this low energy focused ion beam to the one or more one predetermined pattern milling period in the exposure of this semi-manufacture sample thin layer, so that unit area sends the ion of prescribed dose this low energy focused ion beam; And
By one or more exposures of this this semi-manufacture sample thin layer of low energy focused ion beam milling, to remove this breakable layer of at least a portion, produce thus the finished product sample thin layer that comprises this features relevant of at least a portion.
31. computer-readable mediums as claimed in claim 30, wherein, computer instruction causes the computing machine of controlling this focused ion beam system by measuring the beam current of this low energy focused ion beam and determining that the beam current after calibration characterizes the material clearance rate of this low energy focused ion beam.
32. computer-readable mediums as claimed in claim 31, wherein, the dosage of unit area ion depends on the area in region at beam current after this calibration, this pattern place of milling and the predetermined pattern milling time that this low energy focused ion beam is used.
33. computer-readable mediums as claimed in claim 30, wherein, the material clearance rate that computer instruction causes the computing machine of this focused ion beam system of control to measure to property by experiment this low energy focused ion beam characterizes the material clearance rate of this low energy focused ion beam.
34. computer-readable mediums as described in claim 30 to 33 any one, wherein, this high-energy focusing ion beam has the landing energy that is greater than eight kiloelectron-volts (8 keV).
35. computer-readable mediums as described in claim 30 to 33 any one, wherein, this low energy focused ion beam has the landing energy that is less than eight kiloelectron-volts (8 keV).
36. computer-readable mediums as described in claim 30 to 33 any one, further comprise causing and control the computer instruction that the computing machine of this focused ion beam system proceeds as follows:
Produce first group of one or more thin layer, each thin layer in this group receives the ion of the first prescribed dose of this low energy focused ion beam unit area transmission;
Time point in this group thin layer process of milling or one or more features of this first group of thin layer of point in time measurement afterwards;
Record one or more features of this measured first group of thin layer;
Difference based between expection thin layer feature and one or more features of measured this first group of thin layer is calculated the second prescribed dose of the ion of this low energy focused ion beam unit area;
The second pattern milling time of using produces second group of one or more thin layer, to send the second prescribed dose of the ion of this low energy focused ion beam unit area.
37. computer-readable mediums as claimed in claim 36, wherein, personnel manually observe one or more features of this first group of thin layer, and these personnel provide the pondage factor using calculating this second prescribed dose.
38. computer-readable mediums as claimed in claim 36, wherein, one or more features of this first group of thin layer of machine vision algorithm measurement, and one or more features of this measured first group of thin layer are for calculating the pondage factor using when determining this second prescribed dose.
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